HPLC method for detecting genotoxic impurities in candesartan cilexetil

A technology of candesartan medoxomil and a detection method is applied in the field of detection of candesartan cilexetil genotoxic impurity N-nitrosodibutylamine, and can solve the problems of less research on NDBA and the like

Active Publication Date: 2020-11-20
迪嘉药业集团股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many studies on the analy

Method used

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  • HPLC method for detecting genotoxic impurities in candesartan cilexetil
  • HPLC method for detecting genotoxic impurities in candesartan cilexetil
  • HPLC method for detecting genotoxic impurities in candesartan cilexetil

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Preparation of reference solution

[0035] Accurately weigh 150mg of NDBA reference substance, put it in a 10ml volumetric flask, add methanol to dissolve it and set it to volume, shake well, take 1ml precisely, put it in a 100ml volumetric flask, add methanol to dissolve it, set it to volume, shake it up, then take 1ml precisely and put it in 100ml In the volumetric flask, add methanol to dissolve and make up to volume, shake well, and use it as the reference substance stock solution.

[0036] Precisely measure 1ml of the reference substance stock solution, put it in a 10ml measuring bottle, add methanol-water mixed solvent with a volume ratio of 3:7 to dilute to the mark, and shake well to obtain the reference substance solution.

[0037] (2) Preparation of the test solution Precisely weigh 70 mg of the candesartan cilexetil sample (batch number: CA200302A) into a 10 ml measuring bottle, add 5 ml of methanol-water mixed solvent with a volume ratio of 3:7, shake vi...

Embodiment 2

[0058] Example 2. Sample detection

[0059] According to the method described in Example 1, 6 batches of candesartan cilexetil test solution were prepared and injected for detection. The test results are shown in Table 3.

[0060] Table 3 NDBA detection results

[0061]

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Abstract

The invention relates to a method for detecting genotoxic impurities in candesartan cilexetil, and belongs to the technical field of medicine quality control. The detection method comprises the stepsof 1, preparing a reference substance solution; 2, preparing a test solution; 3, preparing a sample adding test solution; 4, taking Thermo Gold C18 as a chromatographic column, taking a methanol-watermixed solution with a volume ratio of 63:37 as a mobile phase A, and taking acetonitrile as a mobile phase B, wherein the detection wavelength is 240nm; introducing a sample and carrying out gradientelution according to a table 1, wherein the flow rate is 1.0 ml/min, the column temperature is 30 DEG C, and the sample size is 80[mu]l; and recording a chromatogram, and calculating the content of the genotoxic impurity NDBA. The invention provides an HPLC/UV detection method of genotoxic impurity NDBA in candesartan cilexetil.

Description

technical field [0001] The invention relates to a method for detecting the genotoxic impurity N-nitrosodibutylamine of candesartan cilexetil, belonging to the technical field of drug quality control. Background technique [0002] Sartan antihypertensive drugs are a new type of drugs with novel mechanism of action, definite curative effect and less adverse reactions. They occupy an important position in the drug market for the treatment of hypertension and have broad prospects for market development. Since N-nitrosodimethylamine (NDMA) was detected in valsartan API in July 2018, various nitrosamine impurities have been detected in other sartan APIs, such as NDMA, N - Nitrosodiethylamine (NDEA) and the like. N-nitrosamine substances are genotoxic impurities, which are clearly indicated in ICHM7 as having high carcinogenicity, and belong to the "concern queue" substances. At present, there are many studies on the analysis of NDMA and NDEA, but less studies on NDBA. In order ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675
Inventor 安宝文曲赛男刘超陈杨刘萍
Owner 迪嘉药业集团股份有限公司
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